CN102674322A - Method for preparing micron graphite powder by using spark plasma - Google Patents
Method for preparing micron graphite powder by using spark plasma Download PDFInfo
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- CN102674322A CN102674322A CN2012101248109A CN201210124810A CN102674322A CN 102674322 A CN102674322 A CN 102674322A CN 2012101248109 A CN2012101248109 A CN 2012101248109A CN 201210124810 A CN201210124810 A CN 201210124810A CN 102674322 A CN102674322 A CN 102674322A
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Abstract
The invention discloses a method for preparing micron graphite powder by using spark plasma. The reaction method comprises the following steps: mainly utilizing the spark plasma generated between natural graphite blocks, generating the plasma under plasma tiny atmosphere, and breaking and peeling off graphite in a high-temperature, high-atmospheric pressure and high-voltage electric filed to obtain the micron graphite powder. Active particles generated in the discharge process of plasma in water can break carbon-carbon bonds on the surface of the graphite and are further oxidized into hydroxyl carboxyl and other functional groups; and moreover, the graphite powder prepared by the method is rich in oxygen-contained functional groups and is easily further oxidized and peeled off to prepare grapheme. Compared with a conventional mechanical grinding method, the method has the advantages of simplicity, quickness, low energy consumption, greenness and environment friendliness.
Description
Technical field
The present invention relates to carbon material, particularly a kind of spark plasma prepares the method for micron graphite powder.
Background technology
Graphite is a kind of crystal habit aggregate of carbon, is the flaky graphite crystal and has the hexaplanar reticulated structure, and carbon atom is the sp by three-fold coordination in the synusia
2The six-membered ring structure that the hydridization carbon atom constitutes has sp in a large number
2When the carbon atom of hybridized orbital mutually combines, sp separately
2The hybridized orbital formation key that mutually combines; Remaining 1 2p electronics formation bonding electron of not participating in hydridization can be done the motion that is parallel to aspect more freely in the stratum reticulare of plane, consequent Van der Waals force makes between the stratum reticulare of plane and combines, and the structure that forms graphite can be found out; The dual combination that has covalent linkage and metallic bond between the carbon atom; Bonding force is very strong, and fusing point is very high, and chemical property is stable; With faint Van der Waals force adjacent lamina is coupled together between stratum reticulare, this makes the reactive force between the adjacent lamina very little, easily relatively sliding between genetic horizon.Because these structural characteristics, Graphite Powder 99 can be used to lubricate, make graphite bomb, guidance agent interfering material, stealth material, hydrogen storage material, field emmision material etc., in addition, still as the main raw material for preparing Graphene.In a word, the Graphite Powder 99 that has various excellent properties is extensively lubricated with chemical industry, iron and steel, space flight and aviation, lubricated wet goods field.
Along with nanotechnology and nano material application and development, micro-nano level Graphite Powder 99 has obtained sufficient research in recent years.The preparation method of micro-nano Graphite Powder 99 roughly is divided into two big types at present: one type is directly or indirectly from natural flake graphite, to obtain, like mechanical milling method, explosion method, supersonic method and electrochemical intercalation method; Another kind of is synthetic by the carbon-rich material preparation, and these class methods have taken place in the preparation process by reconfiguring of atom, like the pulse laser precipitator method, detonation synthesis method, chemical Vapor deposition process and chemical synthesis etc.In first kind method, prepared Graphite Powder 99 is a nanometer scale on thickness, and diameter is relatively large; Second class methods are owing to passed through the permutatation combination of carbon atom, and three dimension scale is less.All have some shortcomings in two class methods, little like productive rate output, time consumption and energy consumption is high, preparation condition harshness etc.And above-mentioned most of method prepares in the Graphite Powder 99 process not to its surface-treated.Because of the big specific surface area of Graphite Powder 99, thereby cause surface energy to be reunited, precipitate, reduced the function of system than big in medium, being prone to, so in the preparation Graphite Powder 99, also will be to its finishing.
The present invention adopts the spark plasma gas to prepare micron order Graphite Powder 99 and other some traditional method ratios, simple and fast, and energy consumption is low, convenient separation, many advantages such as environmental protection have very high using value.
Summary of the invention
The technical problem that the present invention solved provides a kind of green, efficiently utilizes plasma body to prepare the method for micron graphite powder.
For solving the problems of the technologies described above, the concrete scheme that is adopted is following:
Spark plasma prepares the method for micron graphite powder; It is characterized in that: utilize plasma reactor, through preparation micron graphite powder in the natural graphite piece of spark plasma discharge from be submerged in liquid, described spark plasma discharge is voltage 1-20KV; Electric current 1-200 A; Pulse is 10-1000 ns, reacts cumulative time 0.1-100 hour, and reaction conditions is temperature 10-500 ℃.
Described spark plasma prepares the method for micron graphite powder, it is characterized in that: described plasma reactor is the container that there is electrode on both sides.
Described spark plasma prepares the method for micron graphite powder, it is characterized in that: described liquid is nonconducting liquid.
Described spark plasma prepares the method for micron graphite powder, it is characterized in that: described micron graphite powder size is between 0.1-20 um, and thickness is between 10-100 nm.
Prepared Graphite Powder 99 contains functional group's (sample for preparing in the water) such as more hydroxyl carboxyl than ordinary method preparation.
Advantage of the present invention:
The present invention is superior to traditional mechanical mill preparation method, mild condition, and preparation is simple, and particle is littler, and it is low to consume energy, environment-friendly and green.
Description of drawings
The SEM photo of the Graphite Powder 99 that Fig. 1 prepares for different condition.
Fig. 2 is the size distribution of Graphite Powder 99.
Fig. 3 is the XRD figure spectrum of Graphite Powder 99.
Embodiment
Employed reactor drum is that both sides are plate electrodes, and the bottom is a silk screen, the container of insulation sealing all around, and capacity is 0.5-20 L, distance is 10-50 cm between the plate electrode.The hole of silk screen is 0.5-1 mm.
The voltage that produces spark plasma is 1-20KV, and electric current is 1-200 A, and pulse is 10-1000 ns, handles cumulative time 0.1-100 hour.
Embodiment 3
Dull and stereotyped with specific reactor drum, distance is 10 cm between the electrode, and capacity is 0.5 L.The voltage of used plasma body is 10 KV, electric current 120 A, and pulse is 500ns.The flaky graphite piece is roughly 1-5 mm, and weight is 50 g, and deionized water is 150 mL, floods graphite block, and the accumulated discharge time is 20 minutes, obtains about 1.8 g Graphite Powder 99s, and yardstick is the 1-20 micron, and graphite purity is 97.2%.
Dull and stereotyped with specific reactor drum, distance is 10 cm between the electrode, and capacity is 0.5 L.The voltage of used plasma body is 10 KV, electric current 120 A, and pulse is 500ns.The flaky graphite piece is roughly 1-5 mm, and weight is 50 g, and deionized water is 150 mL, floods graphite block, and the accumulated discharge time is 40 minutes, obtains about 3.1 g Graphite Powder 99s, and yardstick is the 1-20 micron.
With specific reactor drum, distance is 10 cm between the plate electrode, and capacity is 0.5 L.The voltage of used plasma body is 10 KV, electric current 120 A, and pulse is 500ns.The flaky graphite piece is roughly 1-5 mm, and weight is 50 g, and deionized water is 150 mL, floods graphite block, and the accumulated discharge time is 60 minutes, obtains about 6.0 g Graphite Powder 99s, and yardstick is the 1-20 micron.
With specific reactor drum, distance is 15 cm between the plate electrode, and capacity is 1 L.The voltage of used plasma body is 15 KV, electric current 100 A, and pulse is 500ns.The flaky graphite piece is roughly 1-5 mm, and weight is 200 g, and deionized water is 300 mL, floods graphite block, and the accumulated discharge time is 20 minutes, obtains about 5.8 g Graphite Powder 99s, and yardstick is the 1-20 micron.
With the reactor drum of comparatively large vol, distance is 15 cm between the plate electrode, and capacity is 2 L.The voltage of used plasma body is 15 KV, electric current 150 A, and pulse is 500ns, power reaches 80% of power supply peak power.The flaky graphite piece is roughly 2-10 mm, and weight is 500 g, and deionized water is 500 mL, and the accumulated discharge time is 40 minutes, obtains about 25.4 g Graphite Powder 99s, and yardstick is the 1-20 micron.
Embodiment 8
With distance between the plate electrode is 10 cm, and capacity is the reactor drum of 0.5L.The voltage of used plasma body is 10KV, electric current 120 A, and pulse is 500ns.The flaky graphite piece is roughly 1-5 mm, and weight is 50 g, and ethanol is 150 mL, floods graphite block, and the accumulated discharge time is 20 minutes, obtains about 2.0 g Graphite Powder 99s, and yardstick is the 2-15 micron, and graphite purity is 97.5%.
Embodiment 9
With distance between the plate electrode is 10 cm, and capacity is the reactor drum of 0.5 L.The voltage of used plasma body is 10KV, electric current 120 A, and pulse is 500ns.The flaky graphite piece is roughly 1-5 mm, and weight is 50 g, and toluene (or other benzene kind solvent) is 150 mL, floods graphite block, and the accumulated discharge time is 20 minutes, obtains about 2.3 g Graphite Powder 99s, and yardstick is the 1-10 micron, and graphite purity is 98.8%.
With distance between the plate electrode is 10 cm, and capacity is the reactor drum of 0.5 L.The voltage of used plasma body is 10KV, electric current 110 A, and pulse is 500ns.The flaky graphite piece is roughly 1-5 mm, and weight is 50 g, and hydrocarbon oil is 150 mL, floods graphite block, and the accumulated discharge time is 20 minutes, obtains about 2.1 g Graphite Powder 99s, and yardstick is the 1-5 micron, and graphite purity is 98.1%.
Claims (4)
1. a spark plasma prepares the method for micron graphite powder; It is characterized in that: utilize plasma reactor, through preparation micron graphite powder in the natural graphite piece of spark plasma discharge from be submerged in liquid, described spark plasma discharge is voltage 1-20KV; Electric current 1-200 A; Pulse is 10-1000 ns, reacts cumulative time 0.1-100 hour, and reaction conditions is temperature 10-500 ℃.
2. spark plasma according to claim 1 prepares the method for micron graphite powder, it is characterized in that: described plasma reactor is the container that there is electrode on both sides.
3. spark plasma according to claim 1 prepares the method for micron graphite powder, it is characterized in that: described liquid is nonconducting liquid.
4. spark plasma according to claim 1 prepares the method for micron graphite powder, it is characterized in that: described micron graphite powder size is between 0.1-20 um, and thickness is between 10-100nm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103484889A (en) * | 2013-09-23 | 2014-01-01 | 无锡源清高新技术研究所有限公司 | Method for preparing high-quality few-layer graphene powder in large scale |
| CN106544689A (en) * | 2016-10-03 | 2017-03-29 | 北京奈艾斯新材料科技有限公司 | A kind of method that utilization mineral carbon prepares nano carbon sol |
| CN107032333A (en) * | 2017-06-15 | 2017-08-11 | 成都新柯力化工科技有限公司 | A kind of method that graphene is prepared based on laser lift-off |
| CN107777674B (en) * | 2017-09-26 | 2019-11-29 | 深圳先进技术研究院 | A method of two-dimensional material is prepared using atmospheric plasma |
| CN114620716A (en) * | 2022-03-25 | 2022-06-14 | 西南交通大学 | Fluorinated graphene and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101029264A (en) * | 2007-04-03 | 2007-09-05 | 张书达 | Modified gear oil |
| CN102324509A (en) * | 2011-09-20 | 2012-01-18 | 北京工业大学 | Preparation method of metastable phase LiC6 alloy |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101029264A (en) * | 2007-04-03 | 2007-09-05 | 张书达 | Modified gear oil |
| CN102324509A (en) * | 2011-09-20 | 2012-01-18 | 北京工业大学 | Preparation method of metastable phase LiC6 alloy |
Non-Patent Citations (2)
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| 胡耀娟等: "石墨烯的制备、功能化及在化学中的应用", 《物理化学学报》 * |
| 郭双全等: "火花等离子体放电制备粉末技术", 《材料导报：综述篇》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103484889A (en) * | 2013-09-23 | 2014-01-01 | 无锡源清高新技术研究所有限公司 | Method for preparing high-quality few-layer graphene powder in large scale |
| CN103484889B (en) * | 2013-09-23 | 2015-11-04 | 无锡源清高新技术研究所有限公司 | A kind of method preparing the few layer graphene powder of high quality in a large number |
| CN106544689A (en) * | 2016-10-03 | 2017-03-29 | 北京奈艾斯新材料科技有限公司 | A kind of method that utilization mineral carbon prepares nano carbon sol |
| CN107032333A (en) * | 2017-06-15 | 2017-08-11 | 成都新柯力化工科技有限公司 | A kind of method that graphene is prepared based on laser lift-off |
| CN107777674B (en) * | 2017-09-26 | 2019-11-29 | 深圳先进技术研究院 | A method of two-dimensional material is prepared using atmospheric plasma |
| CN114620716A (en) * | 2022-03-25 | 2022-06-14 | 西南交通大学 | Fluorinated graphene and preparation method and application thereof |
| CN114620716B (en) * | 2022-03-25 | 2023-02-28 | 西南交通大学 | Fluorinated graphene and preparation method and application thereof |
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